海燕化学成分的分离与鉴定

目的研究海洋生物海燕(Asterina pectinifera)的化学成分。方法采用大孔树脂柱色谱、硅胶柱色谱、凝胶柱色谱、制备薄层色谱、高效液相色谱等手段分离纯化,根据理化性质、波谱分析和文献对照的方法对所分离的化合物进行结构鉴定。结果从海燕体内分离并鉴定了9个化合物,分别为:3-十八烷氧基-1,2-丙二醇[3-(octadecyloxy)-1,2-propanediol,1]、正二十碳酸(arachidic acid,2)、胆甾-7-烯-3β-醇(cholesta-7-ene-3β-ol,3)、尿嘧啶(uracil,4)、5α-胆甾烷-3β,4β,6α,7α,8,15β,16β,26-八醇(5α-cholestane-3β,4β,6α,7α,8,15β,16β,26-octol,5)、5α-胆甾烷-3β,6α,8,15α,24-五醇(5α-cholestane-3β,6α,8,15β,24-pentaol,6)、色氨酸(tryptophan,7)、3,4-二羟基苯甲酸(3,4-dihydroxybenzoic acid,8)、pectinioside B([(5α,20R,22R,23S,24S)-22,23-epoxy-3β,6α,20-trihydroxyergost-(9)11-ene 6-O-{β-D-galactopyranosyl-(1→4)-[β-D-quinovopyranosyl-(1→2)]-β-D-glucopyranosyl-(1→4)-[β-D-quinovopyranosyl-(1→2)]-β-D-xylopyranosyl-(1→3)-β-D-quinovopyranoside}-3-O-sodium sulfate],9)。结论化合物2、8为首次从海燕中分离得到,化合物9为首次从中国海域的海星纲中分离得到。首次采用二维核磁技术确定化合物9的结构,并首次对其1H-NMR数据及二维谱数据进行归属。

Isolation and identification of constituents from Asterina pectinifera

Objective To study the chemical constituents of the starfish Asterina pectinifera. Methods These compounds were isolated by column chromatography on silica gel, sephadex LH-20 and HPLC. Their structures were identified by spectroscopic analysis and physical-chemical properties. Results Nine compounds were obtained and identified as 3-(octadecyloxy)-1,2-propanediol (1), arachidic acid (2), cholesta-7-ene-3β-ol (3), uracil (4), 5α-cholestane-3β, 4β, 6α, 7α, 8, 15β, 16β, 26-octol (5), 5α-cholestane-3β, 6α, 8, 15α, 24-pentaol (6), tryptophan (7),3, 4-dihydroxybenzoic acid (8), (5α, 20R, 22R, 23S, 24S)-22, 23-epoxy-3β, 6α, 20-trihydroxyergost-(9)11-ene 6-O-｛β-D-galactopyranosyl-(1→4)- [ β-D-fucopyranosyl-(1→2)]-β-D-glucopyranosyl-(1→4) -[ β-D-quinovopyranosyl-(1→2)]-β-D- xylopyranosy-l-(1→3)-β-D-quinovopyranoside}-3-O-sodium sulfate (9). Conclusions Compounds 2 and 8 are obtained from Asterina pectinifera for the first time. ¹H-NMR spectroscopic data of compound 9 is reported for the first time and this compound is also identified by 2-D NMR for the first time.